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1,2-Dichloroethane → 4-Amino-3-chlorobenzoic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1,2-Dichloroethane | HCID 11 | — |
| 反応物 | Ethyl 4-amino-3-chlorobenzoate | HCID 1515285 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | 4-Amino-3-chlorobenzoic acid | HCID 17211 | 112.5% |
反応手順
Compound (1) (0.67 g, 5.5 mmol) and EDC (1.1 g, 5. 7 mmol) was dissolved in dimethyl sulfoxide (DMSO) (10 mL). N,N-dimethyl 1,2-ethylenediamine [compound (2)] (7.5 mL, 5.7 mmol) was added and the mixture was stirred at room temperature for 5 hours, whereafter the reaction mixture was freeze dried. The residue was subjected to column chromatography [silicon dioxide (SiO2) plates chromatographed in chloroform (CHCl3)-methanol (30:1, v/v)+triethylamine (Et3N) (1:1, v/v). This procedure gave quantitative yield (1.1 g) of compound (3) as a syrup.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06713517B1 |
| 出典データセット | uspto-grants-2004_03 |
| ORD ID | ord-4b6b63a9481a46e09e5c7d107b9c9d63 |
| 出典メモ | uspto-grants-2004_03 |